# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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data_i4(1)_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H59 B2 Cl2 Cu Mn2 N22 O20.50'
_chemical_formula_weight         1490.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   36.102(6)
_cell_length_b                   36.102(6)
_cell_length_c                   9.930(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12943(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2371
_cell_measurement_theta_min      2.889
_cell_measurement_theta_max      19.3125

_exptl_crystal_description       rod
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6112
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7046
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25740
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_sigmaI/netI    0.1383
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         28.32
_reflns_number_total             7662
_reflns_number_gt                3570
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1134P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7662
_refine_ls_number_parameters     423
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1788
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.2380
_refine_ls_wR_factor_gt          0.1849
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 1.0000 0.5000 0.0000 0.0312(3) Uani 1 2 d S . .
N1 N 0.94733(13) 0.46218(13) 0.0567(5) 0.0347(12) Uani 1 1 d . . .
N2 N 0.94721(12) 0.45093(12) 0.1909(5) 0.0292(11) Uani 1 1 d . . .
C1 C 0.91861(16) 0.44525(16) 0.0035(7) 0.0354(14) Uani 1 1 d . . .
H1 H 0.9120 0.4474 -0.0867 0.043 Uiso 1 1 calc R . .
C2 C 0.91833(16) 0.42875(16) 0.2092(7) 0.0364(15) Uani 1 1 d . . .
H2 H 0.9120 0.4178 0.2908 0.044 Uiso 1 1 calc R . .
N3 N 0.89948(13) 0.42423(14) 0.0939(6) 0.0372(13) Uani 1 1 d . . .
N4 N 1.02780(12) 0.46246(13) 0.1076(5) 0.0327(12) Uani 1 1 d . . .
N5 N 1.01507(12) 0.44934(12) 0.2292(5) 0.0284(11) Uani 1 1 d . . .
C3 C 1.05906(16) 0.44545(16) 0.0870(7) 0.0359(14) Uani 1 1 d . . .
H3 H 1.0738 0.4497 0.0118 0.043 Uiso 1 1 calc R . .
C4 C 1.03989(17) 0.42449(15) 0.2727(7) 0.0359(15) Uani 1 1 d . . .
H4 H 1.0379 0.4113 0.3529 0.043 Uiso 1 1 calc R . .
N6 N 1.06808(13) 0.42116(13) 0.1849(5) 0.0336(12) Uani 1 1 d . . .
N7 N 1.01152(14) 0.47455(13) -0.1785(6) 0.0384(13) Uani 1 1 d . . .
N8 N 1.02071(13) 0.49480(13) -0.2912(5) 0.0322(11) Uani 1 1 d . . .
C5 C 1.0151(2) 0.43983(18) -0.2198(8) 0.0509(19) Uani 1 1 d . . .
H5 H 1.0105 0.4196 -0.1641 0.061 Uiso 1 1 calc R . .
C6 C 1.02975(18) 0.47123(18) -0.3892(7) 0.0445(17) Uani 1 1 d . . .
H6 H 1.0377 0.4784 -0.4743 0.053 Uiso 1 1 calc R . .
N9 N 1.02598(19) 0.43606(16) -0.3502(7) 0.0596(18) Uani 1 1 d . . .
B1 B 0.97770(18) 0.46249(18) 0.2889(7) 0.0290(15) Uani 1 1 d . . .
H1A H 0.9735 0.4523 0.3791 0.035 Uiso 1 1 calc R . .
Mn1 Mn 0.86414(2) 0.37165(2) 0.07845(10) 0.0331(3) Uani 1 1 d . . .
N10 N 0.87460(14) 0.36931(14) -0.1184(6) 0.0415(13) Uani 1 1 d . . .
C7 C 0.90623(19) 0.36215(18) -0.1733(8) 0.0486(18) Uani 1 1 d . . .
H7 H 0.9081 0.3628 -0.2667 0.058 Uiso 1 1 calc R . .
C8 C 0.93893(19) 0.35309(18) -0.0954(10) 0.055(2) Uani 1 1 d . . .
C9 C 0.9728(2) 0.3511(2) -0.1641(11) 0.072(3) Uani 1 1 d . . .
H9 H 0.9735 0.3547 -0.2568 0.086 Uiso 1 1 calc R . .
C10 C 1.0052(2) 0.3439(2) -0.0953(16) 0.097(4) Uani 1 1 d . . .
H10 H 1.0275 0.3427 -0.1415 0.117 Uiso 1 1 calc R . .
C11 C 1.0045(2) 0.3386(2) 0.0382(15) 0.087(4) Uani 1 1 d . . .
H11 H 1.0266 0.3344 0.0837 0.104 Uiso 1 1 calc R . .
C12 C 0.9716(2) 0.3392(2) 0.1101(11) 0.071(3) Uani 1 1 d . . .
H12 H 0.9718 0.3348 0.2024 0.085 Uiso 1 1 calc R . .
C13 C 0.93872(17) 0.34638(18) 0.0447(10) 0.054(2) Uani 1 1 d . . .
O1 O 0.90745(12) 0.34547(12) 0.1204(5) 0.0476(12) Uani 1 1 d . . .
N11 N 0.82098(13) 0.40082(13) 0.0146(5) 0.0350(12) Uani 1 1 d . . .
C14 C 0.79459(17) 0.41333(17) 0.0904(7) 0.0415(16) Uani 1 1 d . . .
H14 H 0.7765 0.4278 0.0496 0.050 Uiso 1 1 calc R . .
C15 C 0.79104(17) 0.40658(17) 0.2336(7) 0.0411(16) Uani 1 1 d . . .
C16 C 0.7579(2) 0.4178(2) 0.2979(9) 0.061(2) Uani 1 1 d . . .
H16 H 0.7404 0.4311 0.2492 0.074 Uiso 1 1 calc R . .
C17 C 0.7511(2) 0.4096(3) 0.4312(9) 0.069(2) Uani 1 1 d . . .
H17 H 0.7291 0.4173 0.4711 0.083 Uiso 1 1 calc R . .
C18 C 0.7768(2) 0.3900(3) 0.5059(9) 0.070(3) Uani 1 1 d . . .
H18 H 0.7718 0.3840 0.5952 0.084 Uiso 1 1 calc R . .
C19 C 0.8096(2) 0.3795(2) 0.4474(7) 0.0516(19) Uani 1 1 d . . .
H19 H 0.8270 0.3668 0.4988 0.062 Uiso 1 1 calc R . .
C20 C 0.81771(17) 0.38748(18) 0.3129(7) 0.0398(15) Uani 1 1 d . . .
O2 O 0.84966(12) 0.37578(12) 0.2614(5) 0.0405(11) Uani 1 1 d . . .
C21 C 0.84233(19) 0.37977(19) -0.2019(7) 0.0478(18) Uani 1 1 d . . .
H21A H 0.8260 0.3587 -0.2136 0.057 Uiso 1 1 calc R . .
H21B H 0.8505 0.3880 -0.2901 0.057 Uiso 1 1 calc R . .
C22 C 0.82247(19) 0.41044(19) -0.1304(7) 0.0466(17) Uani 1 1 d . . .
H22A H 0.8356 0.4336 -0.1430 0.056 Uiso 1 1 calc R . .
H22B H 0.7976 0.4132 -0.1661 0.056 Uiso 1 1 calc R . .
Cl1 Cl 0.89292(6) 0.47002(5) 0.61105(19) 0.0547(5) Uani 1 1 d . . .
O3 O 0.8921(3) 0.4669(3) 0.4718(9) 0.170(4) Uani 1 1 d . . .
O4 O 0.9128(3) 0.5014(2) 0.6306(15) 0.200(6) Uani 1 1 d . . .
O5 O 0.8615(3) 0.4745(2) 0.6817(13) 0.214(7) Uani 1 1 d . . .
O6 O 0.9091(3) 0.4374(2) 0.6523(10) 0.143(3) Uani 1 1 d . . .
O7 O 0.27878(18) 0.99534(17) 0.1030(7) 0.0866(19) Uani 1 1 d . . .
O8 O 0.5388(3) 0.8672(3) 0.0520(10) 0.159(4) Uani 1 1 d . . .
O9 O 0.5000 0.7500 0.1250 0.40(3) Uani 1 4 d S . .
O10 O 0.5935(3) 0.1505(4) 1.0224(10) 0.194(5) Uani 1 1 d . . .
O11 O 0.5121(6) 0.1811(7) 0.0303(17) 0.384(15) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 1.996(5) . ?
Cu1 N4 1.996(5) 9_765 ?
Cu1 N7 2.040(6) . ?
Cu1 N7 2.040(6) 9_765 ?
Cu1 N1 2.408(5) 9_765 ?
Cu1 N1 2.408(5) . ?
N1 C1 1.314(7) . ?
N1 N2 1.393(7) . ?
N2 C2 1.327(7) . ?
N2 B1 1.528(8) . ?
C1 N3 1.363(7) . ?
C2 N3 1.342(8) . ?
N3 Mn1 2.292(5) . ?
N4 C3 1.301(7) . ?
N4 N5 1.376(6) . ?
N5 C4 1.339(7) . ?
N5 B1 1.548(8) . ?
C3 N6 1.349(7) . ?
C4 N6 1.346(8) . ?
N6 Mn1 2.320(5) 15_665 ?
N7 C5 1.325(8) . ?
N7 N8 1.377(7) . ?
N8 C6 1.333(8) . ?
N8 B1 1.543(8) 9_765 ?
C5 N9 1.360(10) . ?
C6 N9 1.335(8) . ?
B1 N8 1.543(8) 9_765 ?
Mn1 O1 1.874(4) . ?
Mn1 O2 1.896(5) . ?
Mn1 N11 1.985(5) . ?
Mn1 N10 1.993(6) . ?
Mn1 N6 2.320(5) 12_756 ?
N10 C7 1.292(8) . ?
N10 C21 1.479(8) . ?
C7 C8 1.449(11) . ?
C8 C9 1.403(10) . ?
C8 C13 1.412(11) . ?
C9 C10 1.378(14) . ?
C10 C11 1.340(15) . ?
C11 C12 1.384(12) . ?
C12 C13 1.379(10) . ?
C13 O1 1.356(9) . ?
N11 C14 1.295(8) . ?
N11 C22 1.482(8) . ?
C14 C15 1.449(10) . ?
C15 C16 1.415(9) . ?
C15 C20 1.422(9) . ?
C16 C17 1.379(11) . ?
C17 C18 1.380(12) . ?
C18 C19 1.375(10) . ?
C19 C20 1.397(9) . ?
C20 O2 1.331(8) . ?
C21 C22 1.498(10) . ?
Cl1 O5 1.345(7) . ?
Cl1 O4 1.356(8) . ?
Cl1 O6 1.376(7) . ?
Cl1 O3 1.387(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N4 180.0(3) . 9_765 ?
N4 Cu1 N7 93.3(2) . . ?
N4 Cu1 N7 86.7(2) 9_765 . ?
N4 Cu1 N7 86.7(2) . 9_765 ?
N4 Cu1 N7 93.3(2) 9_765 9_765 ?
N7 Cu1 N7 180.0(4) . 9_765 ?
N4 Cu1 N1 96.49(17) . 9_765 ?
N4 Cu1 N1 83.51(17) 9_765 9_765 ?
N7 Cu1 N1 83.76(18) . 9_765 ?
N7 Cu1 N1 96.24(18) 9_765 9_765 ?
N4 Cu1 N1 83.51(17) . . ?
N4 Cu1 N1 96.49(17) 9_765 . ?
N7 Cu1 N1 96.24(18) . . ?
N7 Cu1 N1 83.76(18) 9_765 . ?
N1 Cu1 N1 180.0(2) 9_765 . ?
C1 N1 N2 104.3(5) . . ?
C1 N1 Cu1 142.5(4) . . ?
N2 N1 Cu1 113.0(3) . . ?
C2 N2 N1 108.0(5) . . ?
C2 N2 B1 130.1(5) . . ?
N1 N2 B1 121.9(4) . . ?
N1 C1 N3 113.2(6) . . ?
N2 C2 N3 110.8(6) . . ?
C2 N3 C1 103.7(5) . . ?
C2 N3 Mn1 116.1(4) . . ?
C1 N3 Mn1 134.4(4) . . ?
C3 N4 N5 105.4(5) . . ?
C3 N4 Cu1 132.3(4) . . ?
N5 N4 Cu1 122.4(3) . . ?
C4 N5 N4 106.9(5) . . ?
C4 N5 B1 131.7(5) . . ?
N4 N5 B1 121.4(4) . . ?
N4 C3 N6 113.8(6) . . ?
N5 C4 N6 110.9(5) . . ?
C4 N6 C3 103.1(5) . . ?
C4 N6 Mn1 135.8(4) . 15_665 ?
C3 N6 Mn1 121.2(4) . 15_665 ?
C5 N7 N8 103.1(6) . . ?
C5 N7 Cu1 135.6(5) . . ?
N8 N7 Cu1 121.1(4) . . ?
C6 N8 N7 108.3(5) . . ?
C6 N8 B1 129.7(5) . 9_765 ?
N7 N8 B1 121.9(5) . 9_765 ?
N7 C5 N9 114.7(6) . . ?
N8 C6 N9 111.7(7) . . ?
C6 N9 C5 102.1(6) . . ?
N2 B1 N8 108.0(5) . 9_765 ?
N2 B1 N5 107.5(5) . . ?
N8 B1 N5 106.2(5) 9_765 . ?
O1 Mn1 O2 93.3(2) . . ?
O1 Mn1 N11 173.6(2) . . ?
O2 Mn1 N11 92.8(2) . . ?
O1 Mn1 N10 92.2(2) . . ?
O2 Mn1 N10 174.5(2) . . ?
N11 Mn1 N10 81.8(2) . . ?
O1 Mn1 N3 86.47(18) . . ?
O2 Mn1 N3 91.40(19) . . ?
N11 Mn1 N3 91.10(18) . . ?
N10 Mn1 N3 89.7(2) . . ?
O1 Mn1 N6 92.89(18) . 12_756 ?
O2 Mn1 N6 88.21(18) . 12_756 ?
N11 Mn1 N6 89.58(18) . 12_756 ?
N10 Mn1 N6 90.7(2) . 12_756 ?
N3 Mn1 N6 179.23(19) . 12_756 ?
C7 N10 C21 120.7(6) . . ?
C7 N10 Mn1 126.2(5) . . ?
C21 N10 Mn1 113.0(4) . . ?
N10 C7 C8 122.7(7) . . ?
C9 C8 C13 118.4(8) . . ?
C9 C8 C7 117.6(8) . . ?
C13 C8 C7 124.1(6) . . ?
C10 C9 C8 120.5(10) . . ?
C11 C10 C9 120.1(9) . . ?
C10 C11 C12 121.6(9) . . ?
C13 C12 C11 119.9(10) . . ?
O1 C13 C12 116.9(8) . . ?
O1 C13 C8 123.6(6) . . ?
C12 C13 C8 119.5(8) . . ?
C13 O1 Mn1 124.0(4) . . ?
C14 N11 C22 120.6(6) . . ?
C14 N11 Mn1 125.2(5) . . ?
C22 N11 Mn1 114.0(4) . . ?
N11 C14 C15 125.2(6) . . ?
C16 C15 C20 117.5(7) . . ?
C16 C15 C14 118.0(7) . . ?
C20 C15 C14 124.4(6) . . ?
C17 C16 C15 121.5(8) . . ?
C16 C17 C18 120.5(8) . . ?
C19 C18 C17 119.5(8) . . ?
C18 C19 C20 121.8(8) . . ?
O2 C20 C19 118.9(6) . . ?
O2 C20 C15 121.9(6) . . ?
C19 C20 C15 119.2(6) . . ?
C20 O2 Mn1 129.2(4) . . ?
N10 C21 C22 107.4(6) . . ?
N11 C22 C21 107.7(5) . . ?
O5 Cl1 O4 105.7(7) . . ?
O5 Cl1 O6 107.7(6) . . ?
O4 Cl1 O6 116.7(7) . . ?
O5 Cl1 O3 120.8(8) . . ?
O4 Cl1 O3 102.8(8) . . ?
O6 Cl1 O3 103.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.118
_database_code_depnum_ccdc_archive 'CCDC 953714'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_i4(1)_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H42 B2 Cl2 Cu Mn2 N22 O12'
_chemical_formula_weight         1336.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   35.9978(6)
_cell_length_b                   35.9978(6)
_cell_length_c                   9.9081(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12839.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5527
_cell_measurement_theta_min      2.8965
_cell_measurement_theta_max      25.8375

_exptl_crystal_description       rod
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.99
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.39
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5432
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4798
_exptl_absorpt_correction_T_max  0.7276
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25947
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.1146
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.13
_diffrn_reflns_theta_max         28.30
_reflns_number_total             7970
_reflns_number_gt                3287
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1055P)²+33.1866P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7970
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1919
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.2398
_refine_ls_wR_factor_gt          0.1607
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 0.0000 0.0363(3) Uani 1 2 d S . .
N1 N 0.05269(13) 0.03764(14) 0.0464(4) 0.0451(12) Uani 1 1 d . . .
N2 N 0.05489(13) 0.04872(13) 0.1796(4) 0.0399(11) Uani 1 1 d . . .
C1 C 0.08055(17) 0.05472(18) -0.0108(6) 0.0512(16) Uani 1 1 d . . .
H1 H 0.0861 0.0522 -0.1020 0.061 Uiso 1 1 calc R . .
C2 C 0.08366(16) 0.07109(17) 0.1918(6) 0.0467(14) Uani 1 1 d . . .
H2 H 0.0912 0.0818 0.2727 0.056 Uiso 1 1 calc R . .
N3 N 0.10064(14) 0.07647(14) 0.0735(5) 0.0519(13) Uani 1 1 d . . .
N4 N -0.02686(12) 0.03745(13) 0.1131(4) 0.0404(11) Uani 1 1 d . . .
N5 N -0.01285(13) 0.05031(12) 0.2316(4) 0.0388(11) Uani 1 1 d . . .
C3 C -0.05850(17) 0.05419(17) 0.0985(6) 0.0505(16) Uani 1 1 d . . .
H3 H -0.0740 0.0504 0.0248 0.061 Uiso 1 1 calc R . .
C4 C -0.03728(17) 0.07404(17) 0.2802(6) 0.0470(15) Uani 1 1 d . . .
H4 H -0.0344 0.0869 0.3611 0.056 Uiso 1 1 calc R . .
N6 N -0.06670(14) 0.07748(14) 0.1995(5) 0.0518(13) Uani 1 1 d . . .
N7 N -0.01412(13) 0.02635(14) -0.1780(5) 0.0444(12) Uani 1 1 d . . .
N8 N -0.02421(12) 0.00573(13) -0.2882(4) 0.0381(11) Uani 1 1 d . . .
C5 C -0.0167(2) 0.06062(19) -0.2211(7) 0.0601(18) Uani 1 1 d . . .
H5 H -0.0110 0.0809 -0.1668 0.072 Uiso 1 1 calc R . .
C6 C -0.03259(19) 0.02931(19) -0.3876(7) 0.0592(18) Uani 1 1 d . . .
H6 H -0.0405 0.0222 -0.4731 0.071 Uiso 1 1 calc R . .
N9 N -0.02807(18) 0.06436(16) -0.3486(7) 0.0718(17) Uani 1 1 d . . .
B1 B 0.02550(18) 0.03665(19) 0.2837(6) 0.0394(15) Uani 1 1 d . . .
H1A H 0.0310 0.0470 0.3730 0.047 Uiso 1 1 calc R . .
Mn1 Mn 0.13631(3) 0.12910(3) 0.05550(9) 0.0463(3) Uani 1 1 d . . .
N10 N 0.12722(16) 0.13264(15) -0.1411(5) 0.0565(14) Uani 1 1 d . . .
C7 C 0.0960(3) 0.1397(2) -0.1951(8) 0.078(2) Uani 1 1 d . . .
H7 H 0.0947 0.1390 -0.2888 0.093 Uiso 1 1 calc R . .
C8 C 0.0627(3) 0.1488(2) -0.1233(11) 0.084(3) Uani 1 1 d . . .
C9 C 0.0290(3) 0.1505(3) -0.1978(12) 0.112(4) Uani 1 1 d . . .
H9 H 0.0287 0.1468 -0.2907 0.135 Uiso 1 1 calc R . .
C10 C -0.0035(3) 0.1578(3) -0.128(2) 0.147(6) Uani 1 1 d . . .
H10 H -0.0258 0.1585 -0.1753 0.176 Uiso 1 1 calc R . .
C11 C -0.0042(4) 0.1640(4) 0.008(2) 0.152(6) Uani 1 1 d . . .
H11 H -0.0266 0.1693 0.0510 0.182 Uiso 1 1 calc R . .
C12 C 0.0281(3) 0.1626(3) 0.0797(13) 0.120(4) Uani 1 1 d . . .
H12 H 0.0275 0.1666 0.1724 0.144 Uiso 1 1 calc R . .
C13 C 0.0618(2) 0.1552(2) 0.0167(10) 0.079(2) Uani 1 1 d . . .
O1 O 0.09271(13) 0.15567(13) 0.0923(5) 0.0690(13) Uani 1 1 d . . .
N11 N 0.18045(15) 0.10064(15) -0.0061(5) 0.0523(13) Uani 1 1 d . . .
C14 C 0.20709(19) 0.0893(2) 0.0702(7) 0.0617(18) Uani 1 1 d . . .
H14 H 0.2264 0.0766 0.0285 0.074 Uiso 1 1 calc R . .
C15 C 0.2098(2) 0.0943(2) 0.2138(7) 0.066(2) Uani 1 1 d . . .
C16 C 0.2426(2) 0.0846(3) 0.2775(9) 0.102(3) Uani 1 1 d . . .
H16 H 0.2613 0.0731 0.2279 0.122 Uiso 1 1 calc R . .
C17 C 0.2482(3) 0.0915(4) 0.4128(11) 0.135(5) Uani 1 1 d . . .
H17 H 0.2702 0.0846 0.4552 0.162 Uiso 1 1 calc R . .
C18 C 0.2205(3) 0.1088(4) 0.4830(10) 0.136(5) Uani 1 1 d . . .
H18 H 0.2239 0.1138 0.5743 0.163 Uiso 1 1 calc R . .
C19 C 0.1884(3) 0.1188(3) 0.4234(7) 0.105(3) Uani 1 1 d . . .
H19 H 0.1702 0.1305 0.4747 0.127 Uiso 1 1 calc R . .
C20 C 0.1815(2) 0.1120(2) 0.2873(6) 0.066(2) Uani 1 1 d . . .
O2 O 0.14980(13) 0.12374(13) 0.2367(4) 0.0612(12) Uani 1 1 d . . .
C21 C 0.1603(2) 0.1233(2) -0.2198(6) 0.069(2) Uani 1 1 d . . .
H21A H 0.1764 0.1448 -0.2270 0.083 Uiso 1 1 calc R . .
H21B H 0.1532 0.1157 -0.3101 0.083 Uiso 1 1 calc R . .
C22 C 0.1805(2) 0.0925(2) -0.1516(7) 0.070(2) Uani 1 1 d . . .
H22A H 0.1681 0.0690 -0.1689 0.083 Uiso 1 1 calc R . .
H22B H 0.2057 0.0909 -0.1850 0.083 Uiso 1 1 calc R . .
Cl1 Cl 0.39546(7) 0.96662(6) 0.10005(19) 0.0810(6) Uani 1 1 d . . .
O3 O 0.3920(2) 0.9789(3) -0.0248(8) 0.186(4) Uani 1 1 d . . .
O4 O 0.3659(3) 0.9698(2) 0.1824(10) 0.194(5) Uani 1 1 d . . .
O5 O 0.4051(3) 0.9311(2) 0.0982(14) 0.229(6) Uani 1 1 d . . .
O6 O 0.4245(4) 0.9886(4) 0.1511(10) 0.265(8) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.002(4) 9 ?
Cu1 N4 2.002(4) . ?
Cu1 N7 2.066(5) . ?
Cu1 N7 2.066(5) 9 ?
Cu1 N1 2.376(5) . ?
Cu1 N1 2.376(5) 9 ?
N1 C1 1.306(7) . ?
N1 N2 1.381(6) . ?
N2 C2 1.318(7) . ?
N2 B1 1.540(7) . ?
C1 N3 1.354(7) . ?
C2 N3 1.336(7) . ?
N3 Mn1 2.296(5) . ?
N4 C3 1.297(7) . ?
N4 N5 1.359(6) . ?
N5 C4 1.317(7) . ?
N5 B1 1.553(8) . ?
C3 N6 1.338(7) . ?
C4 N6 1.333(7) . ?
N6 Mn1 2.347(5) 15 ?
N7 C5 1.309(8) . ?
N7 N8 1.369(6) . ?
N8 C6 1.335(7) . ?
N8 B1 1.527(8) 9 ?
C5 N9 1.335(8) . ?
C6 N9 1.330(8) . ?
B1 N8 1.527(8) 9 ?
Mn1 O2 1.870(4) . ?
Mn1 O1 1.874(5) . ?
Mn1 N10 1.979(5) . ?
Mn1 N11 1.987(6) . ?
Mn1 N6 2.347(5) 12_666 ?
N10 C7 1.270(9) . ?
N10 C21 1.463(9) . ?
C7 C8 1.432(12) . ?
C8 C13 1.408(12) . ?
C8 C9 1.423(12) . ?
C9 C10 1.384(16) . ?
C10 C11 1.362(19) . ?
C11 C12 1.365(16) . ?
C12 C13 1.392(12) . ?
C13 O1 1.340(9) . ?
N11 C14 1.288(8) . ?
N11 C22 1.471(8) . ?
C14 C15 1.437(9) . ?
C15 C16 1.386(10) . ?
C15 C20 1.404(11) . ?
C16 C17 1.379(13) . ?
C17 C18 1.365(15) . ?
C18 C19 1.348(13) . ?
C19 C20 1.392(9) . ?
C20 O2 1.316(9) . ?
C21 C22 1.486(10) . ?
Cl1 O3 1.319(6) . ?
Cl1 O5 1.326(8) . ?
Cl1 O4 1.345(7) . ?
Cl1 O6 1.404(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N4 180.0(3) 9 . ?
N4 Cu1 N7 87.14(19) 9 . ?
N4 Cu1 N7 92.86(19) . . ?
N4 Cu1 N7 92.86(18) 9 9 ?
N4 Cu1 N7 87.14(18) . 9 ?
N7 Cu1 N7 180.0(4) . 9 ?
N4 Cu1 N1 96.13(17) 9 . ?
N4 Cu1 N1 83.87(17) . . ?
N7 Cu1 N1 95.73(18) . . ?
N7 Cu1 N1 84.27(18) 9 . ?
N4 Cu1 N1 83.87(17) 9 9 ?
N4 Cu1 N1 96.13(17) . 9 ?
N7 Cu1 N1 84.27(18) . 9 ?
N7 Cu1 N1 95.73(18) 9 9 ?
N1 Cu1 N1 180.0(2) . 9 ?
C1 N1 N2 103.6(4) . . ?
C1 N1 Cu1 142.9(4) . . ?
N2 N1 Cu1 113.3(3) . . ?
C2 N2 N1 108.0(4) . . ?
C2 N2 B1 130.6(5) . . ?
N1 N2 B1 121.3(4) . . ?
N1 C1 N3 114.5(5) . . ?
N2 C2 N3 111.6(5) . . ?
C2 N3 C1 102.3(5) . . ?
C2 N3 Mn1 116.3(4) . . ?
C1 N3 Mn1 136.7(4) . . ?
C3 N4 N5 105.3(5) . . ?
C3 N4 Cu1 132.4(4) . . ?
N5 N4 Cu1 122.3(3) . . ?
C4 N5 N4 106.8(5) . . ?
C4 N5 B1 132.6(5) . . ?
N4 N5 B1 120.6(4) . . ?
N4 C3 N6 113.7(5) . . ?
N5 C4 N6 111.8(5) . . ?
C4 N6 C3 102.4(5) . . ?
C4 N6 Mn1 136.4(4) . 15 ?
C3 N6 Mn1 121.0(4) . 15 ?
C5 N7 N8 103.4(5) . . ?
C5 N7 Cu1 136.8(5) . . ?
N8 N7 Cu1 119.8(4) . . ?
C6 N8 N7 107.7(5) . . ?
C6 N8 B1 130.5(5) . 9 ?
N7 N8 B1 121.8(4) . 9 ?
N7 C5 N9 115.2(6) . . ?
N9 C6 N8 111.1(6) . . ?
C6 N9 C5 102.5(6) . . ?
N8 B1 N2 108.8(5) 9 . ?
N8 B1 N5 107.4(5) 9 . ?
N2 B1 N5 107.4(4) . . ?
O2 Mn1 O1 94.8(2) . . ?
O2 Mn1 N10 174.0(2) . . ?
O1 Mn1 N10 91.2(2) . . ?
O2 Mn1 N11 92.0(2) . . ?
O1 Mn1 N11 173.2(2) . . ?
N10 Mn1 N11 82.1(2) . . ?
O2 Mn1 N3 89.17(19) . . ?
O1 Mn1 N3 86.4(2) . . ?
N10 Mn1 N3 92.12(19) . . ?
N11 Mn1 N3 92.62(19) . . ?
O2 Mn1 N6 87.80(18) . 12_666 ?
O1 Mn1 N6 92.6(2) . 12_666 ?
N10 Mn1 N6 91.02(19) . 12_666 ?
N11 Mn1 N6 88.7(2) . 12_666 ?
N3 Mn1 N6 176.72(18) . 12_666 ?
C7 N10 C21 122.8(6) . . ?
C7 N10 Mn1 125.0(6) . . ?
C21 N10 Mn1 112.0(4) . . ?
N10 C7 C8 125.2(8) . . ?
C13 C8 C9 119.0(10) . . ?
C13 C8 C7 123.1(8) . . ?
C9 C8 C7 117.9(10) . . ?
C10 C9 C8 118.0(12) . . ?
C11 C10 C9 122.9(13) . . ?
C10 C11 C12 119.5(14) . . ?
C11 C12 C13 121.1(13) . . ?
O1 C13 C12 118.1(9) . . ?
O1 C13 C8 122.3(8) . . ?
C12 C13 C8 119.6(9) . . ?
C13 O1 Mn1 125.4(5) . . ?
C14 N11 C22 120.8(6) . . ?
C14 N11 Mn1 125.4(5) . . ?
C22 N11 Mn1 113.8(5) . . ?
N11 C14 C15 126.2(7) . . ?
C16 C15 C20 119.9(7) . . ?
C16 C15 C14 118.4(8) . . ?
C20 C15 C14 121.5(7) . . ?
C17 C16 C15 121.3(9) . . ?
C18 C17 C16 118.2(10) . . ?
C19 C18 C17 121.6(10) . . ?
C18 C19 C20 122.1(10) . . ?
O2 C20 C19 117.9(8) . . ?
O2 C20 C15 125.2(6) . . ?
C19 C20 C15 116.9(8) . . ?
C20 O2 Mn1 128.6(4) . . ?
N10 C21 C22 109.1(6) . . ?
N11 C22 C21 107.3(6) . . ?
O3 Cl1 O5 109.5(8) . . ?
O3 Cl1 O4 117.8(7) . . ?
O5 Cl1 O4 107.2(6) . . ?
O3 Cl1 O6 102.7(7) . . ?
O5 Cl1 O6 110.7(9) . . ?
O4 Cl1 O6 108.8(7) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 953715'
